CN102060322A - Method for preparing cubic lead sulfide material - Google Patents
Method for preparing cubic lead sulfide material Download PDFInfo
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- CN102060322A CN102060322A CN 201010153847 CN201010153847A CN102060322A CN 102060322 A CN102060322 A CN 102060322A CN 201010153847 CN201010153847 CN 201010153847 CN 201010153847 A CN201010153847 A CN 201010153847A CN 102060322 A CN102060322 A CN 102060322A
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- based surfactant
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- lead sulfide
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Abstract
The invention provides a method for preparing a lead sulfide material, comprising the following steps of: preparing a reaction mixture of lead nitrate, thiourea and abietyl surfactant according to a molar ratio of (1-2):(2-4):(0.01-0.125), and adding the mixture into a solvent to stir uniformly to obtain a reaction liquid, wherein the mass ratio of the reaction mixture to the solvent is 1;(15-40), and the solvent is selected from one of alcohol and deionized water; and placing the reaction liquid into a sealed high-pressure reaction kettle, heating to 100-180 DEG C, keeping the temperature for 2-8 h, then cooling, cleaning and drying to obtain the lead sulfide material with a particle shape being cubic. Or the reaction liquid is placed into a microwave reactor, the microwave power is controlled to be 50-150W, the reaction temperature is 120-170 DEG C and the reaction time is 1-60 min. Then the lead sulfide material with the particle shape being cubic is obtained after cooling, cleaning and drying.
Description
Technical field
The present invention relates to a kind of method for preparing the lead sulfide material, be specifically related to a kind of method for preparing the lead sulfide material of cube shaped.
Background technology
Lead sulfide is a kind of important semiconductor material, at aspects such as near infrared communication, photoelectric device and solar cells significant application value is arranged.In recent years, it is found that pattern, size and the structure of material directly influence the performance of material, therefore, the special appearance control preparation of material is also become the research focus of field of material preparation.People adopt prepared in various methods to obtain the lead sulfide material of multiple pattern, adopt interpolation tensio-active agent autoclave hydrothermal method to obtain pulmbous sulfide nanospheres (CN101402468A), nanometer rod (CN101049960A), hollow cubic shape nanocrystalline (CN101402467A), single dispersed cubic shape nanocrystalline (CN101402467A), hexagram nanocrystalline (CN101117237A), pyramid rectangular tube (CrystalGrowth﹠amp as people; Design, the 2009,7,3119th page); Utilize microwave assisting method to prepare sexangle, dendroid and ear shape (Materials Letters, the 2009,63,667th page); Utilize the microemulsion auxiliary law to synthesize flower-like nanometer crystalline substance (Solid State Sciences, 2009,11,976-981 page or leaf).In the whole bag of tricks of each bibliographical information, wherein autoclave hydrothermal method processing unit is simple, controls and realize suitability for industrialized production easily, and the microwave method reaction times is short, promptly reacts completely at several minutes or dozens of minutes usually, saves the energy; And auxiliary these methods of tensio-active agent are preferred approach of control material pattern, the tensio-active agent that uses in the above document is Sodium dodecylbenzene sulfonate anion surfactant or hexadecyl trimethyl ammonium bromide cats product or this two kinds of blended tensio-active agents, these two kinds of tensio-active agents are the petroleum chemistry sintetics, and be the chain alkyl structure, have very strong flexibility, have certain defective at control preparation material pattern.Therefore, in petroleum resources exhausted day by day today, it is a kind of inevitable to replace these two kinds of tensio-active agents to become with novel renewable resources derivative tensio-active agent.
Summary of the invention
The invention provides a kind of method for preparing the lead sulfide material, wherein rosin-based surfactant is as the tensio-active agent of control material microscopic appearance.Wherein rosin-based surfactant is to be raw material synthetic product with China's important renewable resources rosin, has raw material and is easy to get, characteristics such as environmental protection.
According to one embodiment of the invention, the method for the lead sulfide material of preparation cube shaped may further comprise the steps:
Reaction mixture according to the mol ratio of 1-2: 2-4: 0.01-0.125 preparation lead nitrate, thiocarbamide, rosin-based surfactant joins this mixture in the solvent, stirs, and obtains reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water;
Reaction solution is put into the autoclave of sealing, be heated to 100-180 ℃, be incubated 2-8 hour, obtain product through overcooling, washing, drying then.
Wherein, autoclave can use reactor well known to those skilled in the art and not have particular requirement.
According to another embodiment of the invention, the method for the lead sulfide material of preparation cube shaped comprises the steps:
Reaction mixture according to the mol ratio of 1-2: 2-4: 0.01-0.125 preparation lead nitrate, thiocarbamide, rosin-based surfactant joins this mixture in the solvent, stirs, and obtains reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water;
Reaction solution is put into microwave reactor, and controlled microwave power is 50-150W, and temperature of reaction is 120-170 ℃, and the reaction times is 1-60min.Obtain product through overcooling, washing, drying then.
The used microwave reactor of the present invention does not have particular requirement, as long as can reach the reaction conditions of the inventive method.
According to one embodiment of the invention, wherein used rosin-based surfactant is selected from one or more in the following table surface-active agent:
Rosin-based surfactant (I)
Wherein, the scope of n is: 1≤n≤6,
Rosin-based surfactant (II)
Wherein, the scope of n is: 1≤n≤4,
Rosin-based surfactant (III)
Wherein, the scope of n is: 1≤n≤10.
Cooling can be naturally cooling, also can be to force cooling.Washing and drying step can adopt various washing drying means well known to those skilled in the art, for example drying can include but not limited to directly the baking oven inner drying, behind suction filtration in baking oven inner drying, infrared drying, microwave drying or the like.
Use the lead sulfide material of scanning electron microscope analysis according to embodiment of the present invention preparation.The length of side that is shaped as of lead sulfide material is the controlled cubes groove of a 0.2-4 μ m shape particle.
Description of drawings
With reference to accompanying drawing and following embodiment, the present invention may be better understood prepares the method for lead sulfide material.
Fig. 1 is lead sulfide particulate scanning electron microscope (SEM) photo for preparing according to one embodiment of present invention;
Fig. 2 is lead sulfide particulate scanning electron microscope (SEM) photo for preparing according to another embodiment of the invention;
Fig. 3 is lead sulfide particulate scanning electron microscope (SEM) photo for preparing according to another embodiment of the invention;
Fig. 4 is lead sulfide particulate scanning electron microscope (SEM) photo for preparing according to another embodiment of the invention.
Embodiment
Embodiment 1
The thiourea solution 4mL, 10g/L rosin-based surfactant A ethanolic soln 0.3mL, the water 0.2mL that get lead nitrate aqueous solution 2mL, the 0.4mol/L of 0.4mol/L join in the reactor, mix, reaction solution is put into 10mL sealing test tube, put into U.S. CE M discover single mold microwave reaction instrument, controlled microwave power 60W, 160 ℃ of temperature of reaction, reaction 5min, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, and dry 8h obtains the cube shaped pulmbous sulfide product of pattern such as Fig. 1 under 80 ℃.
Rosin-based surfactant A
Embodiment 2
The thiourea solution 6mL, the 10g/L rosin-based surfactant A ethanolic soln 0.1mL that get lead nitrate aqueous solution 4mL, the 0.4mol/L of 0.4mol/L add in the reactor, add 1.9mL ethanol, mix, the baking oven that reactor is put into 140 ℃ reacts 4h, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, 80 ℃ down dry 8h obtain the lead sulfide products of pattern such as Fig. 2.
Rosin-based surfactant A
The thiourea solution 4mL, the 10g/L rosin-based surfactant B ethanolic soln 0.1mL that get lead nitrate aqueous solution 2mL, the 0.4mol/L of 0.4mol/L add in the reactor, add 0.4mL ethanol, mix, reaction solution is put into 10mL sealing test tube, put into U.S. CE M discover single mold microwave reaction instrument, controlled microwave power 100W, 130 ℃ of temperature, reaction 10min, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, 80 ℃ down dry 8h obtain the cube shaped pulmbous sulfide products of pattern such as Fig. 3.
Rosin-based surfactant B
Embodiment 4
The thiourea solution 6mL, the 10g/L rosin-based surfactant C ethanolic soln 0.8mL that get lead nitrate aqueous solution 4mL, the 0.4mol/L of 0.4mol/L add in the reactor, add 1.2mL water, mix, the baking oven that reactor is put into 160 ℃ reacts 4h, be cooled to room temperature, with deionized water and washing with alcohol black precipitate each 3 times, centrifugation obtains black precipitate, 80 ℃ down dry 8h obtain the lead sulfide products of pattern such as Fig. 4.
Rosin-based surfactant C
Though above embodiment for example understands specific embodiments of the present invention,, should be understood that these embodiment only are used to illustrate embodiment of the present invention and scope of the present invention are not had any limiting meaning.Claims and any version thereof all should be included in the scope of protection of present invention.
Claims (4)
1. method for preparing the lead sulfide material, may further comprise the steps: the reaction mixture of preparing lead nitrate, thiocarbamide, rosin-based surfactant according to the mol ratio of 1-2: 2-4: 0.01-0.125, this mixture is joined in the solvent, stir, obtain reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water; Reaction solution is put into the autoclave of sealing, be heated to 100-180 ℃, be incubated 2-8 hour, obtaining particle shape through overcooling, washing, drying then is cube shaped lead sulfide material.
2. according to the process of claim 1 wherein, described rosin-based surfactant is selected from any one or its combination of following rosin-based surfactant:
Rosin-based surfactant (I)
Wherein, the scope of n is: 1≤n≤6,
Rosin-based surfactant (II)
Wherein, the scope of n is: 1≤n≤4,
Rosin-based surfactant (III)
Wherein, the scope of n is: 1≤n≤10.
3. method for preparing the lead sulfide material, may further comprise the steps: the reaction mixture of preparing lead nitrate, thiocarbamide, rosin-based surfactant derivative according to the mol ratio of 1-2: 2-4: 0.01-0.125, this mixture is joined in the solvent, stir, obtain reaction solution; Wherein, the mass ratio of reaction mixture and solvent is 1: 15-40, described solvent are selected from a kind of in ethanol and the deionized water; Reaction solution is put into microwave reactor, and controlled microwave power is 50-150W, and temperature of reaction is 120-170 ℃, and the reaction times is 1-60min.Obtaining particle shape through overcooling, washing, drying then is cube shaped lead sulfide material.
4. according to the method for claim 3, wherein used rosin-based surfactant is selected from any one or its combination of following rosin-based surfactant:
Rosin-based surfactant (I)
Wherein, the scope of n is: 1≤n≤6,
Rosin-based surfactant (II)
Wherein, the scope of n is: 1≤n≤4,
Rosin-based surfactant (III)
Wherein, the scope of n is: 1≤n≤10.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101538475A CN102060322B (en) | 2009-11-11 | 2010-04-23 | Method for preparing cubic lead sulfide material |
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| CN200910210835 | 2009-11-11 | ||
| CN200910210835.9 | 2009-11-11 | ||
| CN2010101538475A CN102060322B (en) | 2009-11-11 | 2010-04-23 | Method for preparing cubic lead sulfide material |
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| CN102060322A true CN102060322A (en) | 2011-05-18 |
| CN102060322B CN102060322B (en) | 2012-11-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073053A (en) * | 2013-02-02 | 2013-05-01 | 山东大学 | Method for directly synthesizing lead sulfide cube nano particle film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101452A (en) * | 1952-09-27 | 1978-07-18 | Electronics Corporation Of America | Lead sulfide activation process |
| CN101117237A (en) * | 2007-07-17 | 2008-02-06 | 浙江大学 | Method for preparing hexagon star-shaped plumbous sulfide nanocrystalline |
| CN101544401A (en) * | 2009-04-27 | 2009-09-30 | 杭州电子科技大学 | Method for preparing lead sulfide micron-sized elliptical rings |
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2010
- 2010-04-23 CN CN2010101538475A patent/CN102060322B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101452A (en) * | 1952-09-27 | 1978-07-18 | Electronics Corporation Of America | Lead sulfide activation process |
| CN101117237A (en) * | 2007-07-17 | 2008-02-06 | 浙江大学 | Method for preparing hexagon star-shaped plumbous sulfide nanocrystalline |
| CN101544401A (en) * | 2009-04-27 | 2009-09-30 | 杭州电子科技大学 | Method for preparing lead sulfide micron-sized elliptical rings |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073053A (en) * | 2013-02-02 | 2013-05-01 | 山东大学 | Method for directly synthesizing lead sulfide cube nano particle film |
| CN103073053B (en) * | 2013-02-02 | 2014-07-09 | 山东大学 | Method for directly synthesizing lead sulfide cube nano particle film |
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| CN102060322B (en) | 2012-11-28 |
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